反应详情

温度

50 °C

To a stirred solution of 5′-methyl-3-trifluoromethyl-2′H-[1,4′]bipyrazolyl-3′-ol (Intermediate KA)(270 mg, 1.163 mmol) and cesium carbonate (379 mg, 1.163 mmol) in DMF (2.684 ml) at 50° C. is added 2-bromo-1-(2,4-dichloro-phenyl)-propan-1-one (Intermediate AA) (328 mg, 1.163 mmol) slowly in DMF (1.789 ml). The reaction is stirred at 50° C. for 1 hour before cooling to RT. 2M Na2CO3 (100 ml) is added and the crude product is extracted with EtOAc (2×100 ml). The organic phases are combined, washed with brine, dried over MgSO4 and concentrated in vacuo. The crude product is purified by ISCO combiflash chromatography, eluting with 0 to 100% (iso-hexane/EtOAc) on a 24 g SiO2 column to give the title compound as a light brown oil; MS: m/z 433.24 [M+H]+

1. temperaturebefore cooling to RT
2. extractionthe crude product is extracted with EtOAc (2×100 ml)
3. washwashed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product is purified by ISCO combiflash chromatography
7. washeluting with 0 to 100% (iso-hexane/EtOAc) on a 24 g SiO2 column